Phosphorus-containing Small Rings: X. Phosphorylation of Derivatives of 1-Methyl-2,2-dichlorocyclopropanecarboxylic Acid

Reaction of derivatives of 1-methyl-2,2-dichlorocyclopropanecarboxylic acid with three- and four-coordinate phosphorus acids was studied. It was established that the nucleophilic substitution on the carbonyl carbon atom proceeds without cleavage of the three-membered ring and leads to new types of phosphorus-containing cyclopropanes. The products were found to enhance the germination energy and laboratory germination of cereal, legume, and vegetable seeds.     

Kinetics of Gold Electrodeposition from Cyanide Electrolytes at a Monitored Surface Coverage by Thallium Atoms

A procedure for measuring kinetic parameters of gold electrodeposition in the presence of catalytically active thallium(I) ions while monitoring the coverage of the gold surface by thallium adatoms, , is described. The procedure accounts for the duration of contact between a freshly renewed surface of gold and a thallium-containing solution and assumes that the incorporation rate of thallium adatoms is proportional to and the current density of gold electrodeposition. At = const, kinetic dependences correspond to the Tafel equation. Values of and i ₀ increase with . At = 0.3, 0.6 and i ₀ 3 × 10^–4 A cm^–2, which conforms to values calculated from anodic curves obtained in similar conditions.     

Rapid Determination of Explosives and Narcotics Using a Multicapillary-Column Gas Chromatograph and an Ion-Mobility Spectrometer

A gas chromatograph for the rapid determination of explosives (2,4-dinitrotoluene, 2,4,6-trinitrotoluene, and pentaerythritol tetranitrate) and narcotics (heroin, cocaine hydrochloride, and crack) is described, and its analytical characteristics are presented. The instrument was equipped with a multicapillary column and an ion-mobility spectrometer as a detector.     

Synthesis of 7-formyl-2-methyl-4-oxo-3,4-dihydropyrrolo[3,2-d]-pyrimidine and some other 7-substituted derivatives

A method that utilizes the Vilsmeier reaction to form a pyrrole ring was developed for the preparation of the previously unknown 7-formyl-2-methyl-4-oxo-3,4-dihydropyrrolo[3,2-d]pyrimidine from 2,6-dimethyl-5-amino-4-oxo-3,4-dihydropyrimidine. The nitrile, which was converted to the amide, was obtained from the oxime of the synthesized aldehyde. 7-Unsubstituted pyrrolopyrimidine was synthesized by oxidation of the aldehyde to the corresponding acid and subsequent decarboxylation. The IR and PMR spectroscopic data are presented.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 12, pp. 1672–1674, December, 1977.     

Neutronenabsorption Bei der Aktivierungsanalyse von Kadmium und Kadmiumtellurid

A calculation method of self-shielding coefficients of interesting elements in samples of any forms is given for the neutron activation analysis of cadmium and its compounds. The determination of ten elements in cadmium telluride using radiochemical separation and γ spectrometry is described.      

Preparation and crystal structure of the La2Ni12P5 and isotypic ternary lanthanoid—Nickel phosphides

The new ternary phosphide La₂Ni₁₂P₅ has been prepared by direct arc melting of the components as pure metals and red phosphorus. The crystal structure has been determined using X-ray single crystal diffraction data. The compound exhibits a new type of crystal structure, P2₁/m with lattice parameters a = 10.911(3), b = 3.696(2), c = 13.174(4) Å, β = 108.02(2)°, V = 505,2(6) ų, Z = 2. Atomic parameters least squares refinement of 116 independent variables (anisotropic approximation for thermal vibrations) employed 1 284 independent I_o(hkl); R_F = 0.0278 and R_W = 0.0287. The crystal structure is characterized by trigonal prismatic arrangement of phosphorus atoms stacking variant of infinite (with phosphorus centered) columns built by metal trigonal prisms ‖ [010]. Two or three such columns are connected through common edges (lanthanum atoms). The compounds RE₂Ni₁₂P₅ (where RE = Ce, Pr, Nd and Eu) display the same with La₂Ni₁₂P₅ crystal structure. Lattice parameters of these compounds have been refined using powder diffraction data.     

Kinetics of the reaction of C6H5 with HBr

The rate constant for the reaction of phenyl radical with hydrogen bromide has been measured with the cavity-ring-down method at six temperatures between 297 and 523 K. The Arrhenius expression for the H abstraction reaction can be effectively given by: . The values of these parameters are similar to those for the H + HBr reaction, but are in sharp contrast to those for alkyl radical reactions. The gross difference between the alkyl radical reactions and the phenyl and H-atom reactions could be rationalized in terms of the inductive effects of these radicals as measured by Taft's σ* (polar) constants. © 1993 John Wiley & Sons, Inc.     

Synthesis of 1-alkyl(aralkyl)-4-acyl-2-piperazinones

1-Alkyl(aralkyl)-4-acyl-2-piperazinones are formed in high yields during selective acylation of N-monosubstituted ethylenediamines by benzoyl and cyclohexylcarbonyl chlorides in the presence of pyridine hydrochloride and treatment of the reaction products with chloroacetyl chloride in the presence of potassium tert-butylate.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 514–517, April, 1986.     

Synthesis and Structure of Triphenylbismuth Bis(Fluorobenzoates)

The reaction between triphenylbismuth, hydrogen peroxide, and 3,4,5-trifluorobenzoic or pentafluorobenzoic acid (molar ratio 1 : 1 : 2, respectively) in ether gave triphenylbismuth bis(3,4,5-trifluorobenzoate) (I) and triphenylbismuth bis(pentafluorobenzoate) (II) in 74 and 89% yields, respectively. The structures of compounds I and II were established by X-ray diffraction. The Bi atoms have a distorted trigonal-bipyramidal coordination with acylate groups in the axial positions. The OBiO angles are 170.2(2)° and 171.5(2)° in I and II, respectively. The Bi–C(Ph)_eq bond lengths vary in the range of 2.187(6)–2.204(5) Å, the Bi–O(acyl) lengths are 2.256(5) Å in I, and 2.281(5) and 2.318(5) Å in II. In the crystals I and II, the Bi and carbonyl O atoms are involved in intramolecular interactions (Bi···O(=C) 2.926(5)–3.176(5) Å), which increase the equatorial CBiC angles on the side of these contacts to 136.2(3)° and 138.6(2)° in I and II, respectively.